Scientists have been paying a special atention for the synthesis of one-dimensional D) morphologies to atain new phenomena and novel physicochemical characteristics of materials. Furthermore, D nanostructures exhibit long axial ratio, which has a great inluence on the physical and chemical properties of materials. It is worth mentioning that electrospinning is one of the most common and eicient techniques used for the preparation of D polymer composite nanoibers. Using electrospinning, nanoibers were fabricated by electrostatic stretching of polymer viscous solution by applying a high voltage. This chapter discusses the synthesis of metal oxide nanoibers such as tin oxide SnO 2 ), zinc oxide ZnO), titanium oxide TiO 2 ), and nickel oxide NiO) using electrospinning process of polymer solution containing metal precursors and followed by annealing procedures to eliminate the polymer galleries, which were chosen as a sacriicial template for the preparation of metal oxide nanoibers. SEM, XRD, and XPS are equipped to characterize the electrospun metal oxide nanoibers and the results setle the formation of homogeneously distributed metal oxide nanoibers.